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WO2009014229A1 - Procédé d'activation d'un catalyseur pour la production de chlore - Google Patents

Procédé d'activation d'un catalyseur pour la production de chlore Download PDF

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Publication number
WO2009014229A1
WO2009014229A1 PCT/JP2008/063462 JP2008063462W WO2009014229A1 WO 2009014229 A1 WO2009014229 A1 WO 2009014229A1 JP 2008063462 W JP2008063462 W JP 2008063462W WO 2009014229 A1 WO2009014229 A1 WO 2009014229A1
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WO
WIPO (PCT)
Prior art keywords
catalyst
gas
contact
contact treatment
temperature
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
Application number
PCT/JP2008/063462
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English (en)
Japanese (ja)
Inventor
Youhei Uchida
Kohei Seki
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Sumitomo Chemical Co Ltd
Original Assignee
Sumitomo Chemical Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Sumitomo Chemical Co Ltd filed Critical Sumitomo Chemical Co Ltd
Priority to EP08791701A priority Critical patent/EP2181764A4/fr
Priority to KR1020107003531A priority patent/KR101493545B1/ko
Priority to CN2008801001038A priority patent/CN101754808B/zh
Priority to BRPI0814117-7A2A priority patent/BRPI0814117A2/pt
Priority to US12/669,757 priority patent/US20100183499A1/en
Publication of WO2009014229A1 publication Critical patent/WO2009014229A1/fr
Anticipated expiration legal-status Critical
Priority to US13/362,053 priority patent/US8318125B2/en
Ceased legal-status Critical Current

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Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/90—Regeneration or reactivation
    • B01J23/96—Regeneration or reactivation of catalysts comprising metals, oxides or hydroxides of the noble metals
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J38/00—Regeneration or reactivation of catalysts, in general
    • B01J38/04—Gas or vapour treating; Treating by using liquids vaporisable upon contacting spent catalyst
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J38/00—Regeneration or reactivation of catalysts, in general
    • B01J38/04—Gas or vapour treating; Treating by using liquids vaporisable upon contacting spent catalyst
    • B01J38/10—Gas or vapour treating; Treating by using liquids vaporisable upon contacting spent catalyst using elemental hydrogen
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J38/00—Regeneration or reactivation of catalysts, in general
    • B01J38/04—Gas or vapour treating; Treating by using liquids vaporisable upon contacting spent catalyst
    • B01J38/12—Treating with free oxygen-containing gas
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B7/00—Halogens; Halogen acids
    • C01B7/01—Chlorine; Hydrogen chloride
    • C01B7/03—Preparation from chlorides
    • C01B7/04—Preparation of chlorine from hydrogen chloride
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
    • B01J21/02—Boron or aluminium; Oxides or hydroxides thereof
    • B01J21/04—Alumina
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
    • B01J21/06—Silicon, titanium, zirconium or hafnium; Oxides or hydroxides thereof
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
    • B01J21/06—Silicon, titanium, zirconium or hafnium; Oxides or hydroxides thereof
    • B01J21/063—Titanium; Oxides or hydroxides thereof
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
    • B01J23/40—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals of the platinum group metals
    • B01J23/46—Ruthenium, rhodium, osmium or iridium
    • B01J23/462—Ruthenium
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
    • B01J37/0009—Use of binding agents; Moulding; Pressing; Powdering; Granulating; Addition of materials ameliorating the mechanical properties of the product catalyst
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
    • B01J37/02—Impregnation, coating or precipitation
    • B01J37/0201—Impregnation
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00—Technologies relating to chemical industry
    • Y02P20/50—Improvements relating to the production of bulk chemicals
    • Y02P20/584—Recycling of catalysts

Definitions

  • the present invention relates to a method for activating a catalyst for producing chlorine by oxidizing hydrogen chloride with oxygen.
  • the present invention also relates to a method for producing chlorine by oxidizing hydrogen chloride with oxygen using a catalyst activated by this method.
  • Japanese Patent Application Laid-Open No. 2007-075 21 discloses that a catalyst with reduced activity is substantially oxygen and / or Describes a method of contacting with a gas consisting only of an inert gas. Disclosure of the invention
  • An object of the present invention is to provide a method capable of effectively recovering the activity of a catalyst having decreased activity.
  • the present invention relates to a method for activating a catalyst for producing chlorine by oxidizing hydrogen chloride with oxygen, wherein the catalyst having reduced activity is contact-treated with a reducing gas containing carbon monoxide and Z or hydrogen.
  • the present invention provides a method for activating a catalyst for producing chlorine characterized by
  • the present invention also provides a method for producing chlorine by oxidizing hydrogen chloride with oxygen in the presence of the catalyst activated by the above method.
  • the catalyst targeted by the activation treatment of the present invention is a catalyst used for producing chlorine by oxidizing hydrogen chloride with oxygen (hereinafter sometimes simply referred to as a catalyst).
  • the catalyst include a copper catalyst, a chromium catalyst, and a ruthenium catalyst.
  • the copper catalyst include a catalyst generally referred to as a Deacon catalyst, which is obtained by adding various compounds as the second component to copper chloride and a salting power rhodium.
  • Preferable examples of the chromium catalyst include JP-A-61-136902, JP-A-61-2725105, JP-A-62-113701, and JP-A-6-1.
  • Examples thereof include a catalyst containing chromium oxide as disclosed in JP-A-62-270405. Further, as preferable examples of the ruthenium catalyst, JP-A-9-67110, JP-A-10-338502, JP20000-281314, JP2002-79093A are disclosed. And a catalyst containing ruthenium oxide as disclosed in JP-A 2 002-292227.
  • the method of the present invention is suitably used for a ruthenium catalyst, particularly a catalyst containing ruthenium oxide.
  • the catalyst containing ruthenium oxide may be, for example, substantially composed of only ruthenium oxide, or ruthenium oxide is supported on a support such as alumina, titania, silica, zirconia, niobium oxide, activated carbon and the like. It may be a supported ruthenium oxide, or a complex oxide composed of ruthenium oxide and other oxides such as alumina, titania, silica, zirconia, niobium oxide and the like.
  • the production of chlorine using a catalyst as described above is usually performed continuously under gas phase conditions while supplying hydrogen chloride and oxygen into a fixed bed reactor packed with the catalyst or a fluidized bed reactor in which the catalyst is fluidized. Done in the formula.
  • the reaction temperature is usually 100 to 500, preferably 200 to 400, and the reaction pressure is usually about 0.1 to 5 MPa.
  • oxygen source air or pure oxygen may be used. In order to completely oxidize hydrogen chloride to chlorine, theoretically, 14 mol of oxygen is required for 1 mol of hydrogen chloride. 0.1 to 10 times the stoichiometric amount of oxygen is used.
  • the supply rate of hydrogen chloride is usually about 10 to 200 IT 1 in terms of the volume supply rate of gas per catalyst layer volume (0 ° C, converted to 1 atm), that is, GHSV.
  • Examples of the hydrogen chloride-containing gas that can be used as a hydrogen chloride source include a gas generated by the reaction of hydrogen and chlorine 5, a gas generated by heating hydrochloric acid, and a chlorinated compound.
  • the catalyst activity gradually decreases as the operation time elapses, that is, as the catalyst usage time elapses.
  • unscheduled decline in catalyst activity may occur due to operational mistakes during operation or equipment malfunctions. For example, if it becomes difficult to control the reaction temperature and the catalyst is exposed to high temperature for a long time, or the supply of oxygen is stopped and the catalyst is in contact with hydrogen chloride for a long time in the absence of oxygen,
  • the activity of the catalyst may be reduced. Furthermore, even if the start of oxygen supply is delayed during start-up, or when the reaction is temporarily stopped, the supply stop of hydrogen chloride is delayed, so that even if the catalyst contacts hydrogen chloride in the absence of oxygen for a long time.
  • the activity of the catalyst may decrease.
  • the gas generated by the oxidation reaction is washed and dehydrated with concentrated sulfuric acid, and then the chlorine is separated. The remaining gas (residual gas) is recovered as a raw material and used again for the oxidation reaction. However, if the residual gas contains sulfur, the catalytic activity may be reduced.
  • hydrogen chloride produced as a by-product when an amine is reacted with phosgene to produce an isocyanate may contain impurities such as phosgene-derived sulfide power sulfonyl, hydrogen sulfide, carbon disulfide, and sulfur oxide.
  • the catalytic activity may be lowered. Therefore, in the present invention, the catalytic treatment is performed with a reducing gas containing carbon monoxide and Z or hydrogen in order to recover the activity of the catalyst whose activity has been reduced in this way.
  • the present invention is preferably employed for a catalyst whose activity is reduced as a result of using hydrogen chloride containing sulfur as a raw material in the oxidation reaction among the catalysts whose activity is reduced.
  • the reducing gas containing carbon monoxide and Z or hydrogen may be a gas consisting only of carbon monoxide, a gas consisting only of hydrogen, or a mixed gas of carbon monoxide and hydrogen.
  • an inert gas may be included.
  • the inert gas here is a neutral component which does not substantially oxidize and reduce with respect to the catalyst, and does not substantially exhibit acidity or basicity.
  • water vapor, nitrogen, argon, Helium, carbon dioxide and the like can be mentioned, and two or more of them can be mixed and used as necessary. Nitrogen is preferably used as such an inert gas.
  • the concentration of carbon monoxide and / or hydrogen in the reducing gas is usually 0.1 to 100% by volume, preferably 1 to 20% by volume. If the concentration is low, it takes a long time to activate the catalyst.
  • the temperature at which the catalyst having reduced activity is contact-treated with the reducing gas is usually from 100 to 500, preferably from 150 to 45. It is. If this temperature is too low, it takes a long time to activate the catalyst, and if this temperature is too high, the catalyst components tend to volatilize.
  • the pressure during the contact treatment with the reducing gas is usually from 0.1 to 3 MPa, preferably from 0.1 to 1 MPa.
  • the contact treatment with the reducing gas may be performed in a fixed bed format or a fluidized bed format.
  • the feed rate of the reducing gas, volumetric feed rate of gas per volume of catalyst layer (at 0, in terms of 1 atm.), That is expressed by GHSV, is usually 1 ⁇ 1 0 0 0 0 0 h one about one .
  • the time for contact treatment with the reducing gas is usually 0.5 to It is about 100 hours.
  • an oxidizing gas is a gas containing an oxidizing substance, and typically includes an oxygen-containing gas.
  • oxygen source air or pure oxygen is usually used, and it can be diluted with the above-described inert gas as necessary.
  • nitrogen is preferably used.
  • the oxygen concentration in the gas is usually from 0.1 to 100% by volume, preferably from 10 to L0% by volume.
  • the contact treatment temperature with the oxidizing gas is usually from 200 to 500, and preferably from 25 to 45. If this temperature is too low, it takes a long time to activate the catalyst, and if this temperature is too high, the catalyst components tend to volatilize.
  • the pressure for the contact treatment with the oxidizing gas is usually 0.1 to 3 MPa, preferably 0.1 to IMP a.
  • the contact treatment with the oxidizing gas may be performed in a fixed bed format or a fluidized bed format.
  • the above-mentioned oxidizing gas supply rate is the volume supply rate of the gas per volume of the catalyst layer (0 ° C, converted to 1 atm), that is, expressed as GHSV, usually about 1 to 1 00 0 0 0 O h 1 is there.
  • the time for the contact treatment with the oxidizing gas is usually about 0.5 to 100 hours.
  • a catalyst with reduced activity is contact-treated with water, then contact-treated with the reducing gas, and then contact-treated with the oxidizing gas, or (2) a catalyst with reduced activity is contacted.
  • contact treatment with the reducing gas contact treatment with water and then contact treatment with the oxidizing gas, or (3) contact treatment of the catalyst with reduced activity with the reducing gas.
  • the catalyst can be more effectively activated.
  • the method (1) is more preferable.
  • the water used in the above contact treatment with water is preferably high-purity water such as distilled water, ion-exchanged water, or ultrapure water. If the water used contains a large amount of impurities, such impurities may adhere to the catalyst, and the activity of the catalyst may not be fully activated. However, hydrogen chloride may be dissolved in the water used.
  • the contact treatment temperature with water is usually 0 to 100 ° C, preferably 10 to 90 ° C. If this temperature is too low, the catalyst may not be sufficiently activated.
  • the pressure for the contact treatment with water is usually 0.1 lMPa, preferably atmospheric pressure.
  • the contact treatment with water may be performed in a fixed bed format or a patch batch method.
  • the above water supply rate is the volume supply rate of the liquid per catalyst volume (0 ° C, converted to 1 atm), that is, expressed in LHSV. is about one 1
  • contact treatment time is usually 0.5 5 about 100 hours.
  • water may be circulated.
  • the amount of water used in the batch batch method is usually about 1 to 100 parts by weight per 1 part by weight of the catalyst, and the contact treatment time is usually about 0.5 to 120 hours. .
  • the number of contact treatments is usually about 1 to 10 times.
  • the catalyst thus activated can be reused in the reaction of oxidizing hydrogen chloride with oxygen.
  • the catalyst cost can be reduced, and chlorine can be produced advantageously in terms of cost.
  • the oxidation reaction is carried out while supplying a raw material gas consisting of hydrogen chloride and oxygen into a reactor filled with the catalyst, and the catalyst is not sufficiently continually operated.
  • the activity decreases, the supply of the raw material gas is stopped, and then the activation treatment of the present invention is performed while the catalyst is filled in the reactor, and then the supply of the raw material gas is resumed to perform the oxidation reaction.
  • a prescription in which the activation treatment and the oxidation reaction are repeated is advantageously employed.
  • the gas supply rate (ml l m i n) is 0 and converted to 1 atm unless otherwise specified.
  • titanium oxide [STR-60 R, 100% rutile type, manufactured by Sakai Chemical Co., Ltd.] 100 parts by weight of ⁇ -alumina [AE S-12, manufactured by Sumitomo Chemical Co., Ltd.], 13.2 weights of titania sol 2 parts by weight [Metro Cell 65 SH-4000, manufactured by Shin-Etsu Chemical Co., Ltd.], and then purified water And kneaded.
  • This mixture was extruded into a cylindrical shape having a diameter of 3. ⁇ , dried, and then crushed to a length of about 4 to 6 mm.
  • the obtained molded body was fired in air at 800 ° C. for 3 hours to obtain a carrier made of a mixture of titanium oxide and ⁇ -alumina.
  • This carrier is impregnated with an aqueous solution of ruthenium chloride, dried, and then calcined in air at 250 ° C. for 2 hours, whereby ruthenium oxide is supported on the carrier at a loading ratio of 2% by weight.
  • a supported ruthenium oxide was obtained.
  • this supported ruthenium oxide (new catalyst) was analyzed by ICP emission spectrometry, the sulfur content was 0.02% by weight.
  • the new catalyst obtained in Reference Example 1 (a) was charged into the reactor.
  • a deterioration catalyst was prepared by performing an oxidation reaction while supplying a raw material gas composed of hydrogen chloride (containing 130 vol p pb of sulfur) and oxygen to the reactor.
  • the sulfur content was 0.14% by weight.
  • the deterioration catalyst lg of Reference Example 1 (b) was filled in a nickel reaction tube with an inner diameter of 13 mm, and further as a preheating layer on the gas inlet side of the catalyst layer. Filled.
  • supply of nitrogen gas was stopped, carbon monoxide gas was changed to 3.2 m 1 / min (0.009 mol / h), and nitrogen gas was changed to 28.8 ml / min (0.08 mol). ⁇ / h) and supplied for 2 hours.
  • Hydrogen chloride conversion (%) [Chlorine production rate (mo 1/1) X 2 ⁇ Hydrogen chloride feed rate (mo 1 Zh)] X 100
  • the supply of oxygen is stopped, the supply of nitrogen is set to 80 m 1 Zm in (0.2 2 mo 1 /), and then the temperature of the catalyst layer is changed to 28 1 ⁇ 282 ° C.
  • hydrogen chloride gas (containing 19 volume ppb of sulfur content) is 8 Om 1 / min (0.2 2 mo 1 / h), and oxygen gas is 4 Om 1 Zm in
  • the oxidation reaction was carried out at a catalyst layer temperature of 281 to 282 ° C.
  • Example 2 (a) In the contact treatment with the reducing gas in Example 2 (a), the catalyst activation treatment was performed under the same conditions as in Example 2 (a) except that the temperature of the catalyst layer was changed to 300 ° C.
  • Example 2 (a) In the contact treatment with the reducing gas in Example 2 (a), the catalyst activation treatment was performed under the same conditions as in Example 2 (a) except that the temperature of the catalyst layer was changed to 400 ° C.
  • Example 2 the activated catalyst was evaluated in the same manner as in Example 2 (b). The results are shown in Table 1. The catalyst after this evaluation was analyzed by ICP emission spectrometry, and the sulfur content was 0.08% by weight.
  • Example 2 the activated catalyst was evaluated in the same manner as in Example 2 (b). The results are shown in Table 1. The catalyst after this evaluation was analyzed by ICP emission spectrometry, and the sulfur content was 0.12% by weight.
  • Example 2 (a) In the contact treatment with the reducing gas in Example 2 (a), the temperature of the catalyst layer was set to 300 ° C, and in the contact treatment with the oxidizing gas in Example 2 (a), the temperature of the catalyst layer was set to 400 ° C. Except for the above, the catalyst activation treatment was performed under the same conditions as in Example 2 (a).
  • Example 2 (a) In the contact treatment with the oxidizing gas in Example 2 (a), the catalyst activation treatment was performed under the same conditions as in Example 2 (a) except that the temperature of the catalyst layer was set to 400. (b) Evaluation of activated catalyst
  • Example 2 (a) In the contact treatment with the reducing gas in Example 2 (a), the temperature of the catalyst layer was set to 400 ° C, and in the contact treatment with the oxidizing gas in Example 2 (a), the temperature of the catalyst layer was set to 400 ° C. Except for the above, the catalyst activation treatment was performed under the same conditions as in Example 2 (a).
  • Example 9 (a) In the contact treatment with the reducing gas in Example 9 (a), the catalyst was activated under the same conditions as in Example 9 (a), except that the temperature of the catalyst layer was 200 and the holding time was 2 hours. Processed.
  • Example 9 (a) In the contact treatment with the reducing gas in Example 9 (a), the catalyst activation treatment was performed under the same conditions as in Example 9 (a), except that the temperature of the catalyst layer was 250 ° C.
  • Example 2 the activated catalyst was evaluated in the same manner as in Example 2 (b). The results are shown in Table 1. The catalyst after this evaluation was analyzed by ICP emission spectrometry, and the sulfur content was 0.09% by weight.
  • Example 9 (a) In the contact treatment with the reducing gas in Example 9 (a), the catalyst activation treatment was performed under the same conditions as in Example 9 (a) except that the temperature of the catalyst layer was 400 ° C. (b) Evaluation of activated catalyst
  • Example 9 (a) In the contact treatment with the reducing gas in Example 9 (a), the temperature of the catalyst layer was set to 400 ° C, and in the contact treatment with the oxidizing gas in Example 9 (a), the temperature of the catalyst layer was set to 400 ° C. Except for the above, the catalyst activation treatment was performed under the same conditions as in Example 9 (a).
  • the deterioration catalyst lg of Reference Example 1 (b) was filled in a nickel reaction tube with an inner diameter of 13 mm, and ⁇ -alumina spheres [Nitsukato Co., Ltd.] were used as a preheating layer on the gas inlet side of the catalyst layer.
  • Comparative example 4 (only contact treatment with water is performed as activation treatment)
  • Example 14 The water treatment catalyst lg of 4 (a) was filled in a nickel reaction tube having an inner diameter of 13 mm, and ⁇ -alumina spheres [Nitsukato Co., Ltd.] were used as a preheating layer on the gas inlet side of the catalyst layer.
  • SSA 9 9 5] 1 2 g made.
  • the temperature of the catalyst layer was adjusted to 281 to 282 ° C.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Inorganic Chemistry (AREA)
  • Catalysts (AREA)

Abstract

L'invention porte sur un procédé pour activer un catalyseur pour la production de chlore, suivant lequel un catalyseur à activité diminuée est soumis à un traitement de contact avec un gaz réducteur qui contient du monoxyde de carbone et/ou de l'hydrogène. Le catalyseur peut être activé de façon plus efficace en étant soumis à un traitement de contact avec un gaz oxydant après le traitement de contact avec l'agent réducteur. Comme catalyseur pour la production de chlore, un catalyseur au ruthénium, en particulier un catalyseur contenant de l'oxyde de ruthénium, est activé de façon appropriée par ce procédé.
PCT/JP2008/063462 2007-07-23 2008-07-18 Procédé d'activation d'un catalyseur pour la production de chlore Ceased WO2009014229A1 (fr)

Priority Applications (6)

Application Number Priority Date Filing Date Title
EP08791701A EP2181764A4 (fr) 2007-07-23 2008-07-18 Procédé d'activation d'un catalyseur pour la production de chlore
KR1020107003531A KR101493545B1 (ko) 2007-07-23 2008-07-18 염소를 제조하기 위한 촉매의 부활 방법
CN2008801001038A CN101754808B (zh) 2007-07-23 2008-07-18 用于制造氯的催化剂的活化方法
BRPI0814117-7A2A BRPI0814117A2 (pt) 2007-07-23 2008-07-18 Método para ativar catalisador para produção de cloro
US12/669,757 US20100183499A1 (en) 2007-07-23 2008-07-18 Method for activating catalyst for chlorine production
US13/362,053 US8318125B2 (en) 2007-07-23 2012-01-31 Method for activating catalyst for chlorine production

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
JP2007-190523 2007-07-23
JP2007190523A JP5169047B2 (ja) 2007-07-23 2007-07-23 塩素の製造方法

Related Child Applications (2)

Application Number Title Priority Date Filing Date
US12/669,757 A-371-Of-International US20100183499A1 (en) 2007-07-23 2008-07-18 Method for activating catalyst for chlorine production
US13/362,053 Division US8318125B2 (en) 2007-07-23 2012-01-31 Method for activating catalyst for chlorine production

Publications (1)

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WO2009014229A1 true WO2009014229A1 (fr) 2009-01-29

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US (2) US20100183499A1 (fr)
EP (1) EP2181764A4 (fr)
JP (1) JP5169047B2 (fr)
KR (1) KR101493545B1 (fr)
CN (1) CN101754808B (fr)
BR (1) BRPI0814117A2 (fr)
WO (1) WO2009014229A1 (fr)

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP5189954B2 (ja) * 2008-10-30 2013-04-24 住友化学株式会社 塩素の製造方法
US9610567B2 (en) * 2008-12-30 2017-04-04 Basf Se Process for regenerating a catalyst comprising ruthenium oxide for the oxidation of hydrogen chloride
JP5368883B2 (ja) * 2009-05-29 2013-12-18 住友化学株式会社 塩素製造用触媒の賦活方法および塩素の製造方法
JP2010274216A (ja) * 2009-05-29 2010-12-09 Sumitomo Chemical Co Ltd 塩素製造用触媒の賦活方法および塩素の製造方法
WO2010142604A1 (fr) * 2009-06-10 2010-12-16 Basf Se Procédé d'oxydation de gaz chlorhydrique sur un catalyseur à faible rugosité superficielle
JP5273311B2 (ja) * 2010-09-10 2013-08-28 東亞合成株式会社 セラミック成形用添加剤
EP3756758B1 (fr) * 2019-04-30 2024-05-01 Dalian Institute of Chemical Physics, Chinese Academy of Sciences Catalyseur pour la préparation de chlorure de vinyle par craquage de 1,2-dichloroéthane et procédés de préparation et de régénération associés
CN112916053A (zh) * 2019-12-06 2021-06-08 中国科学院大连化学物理研究所 一种催化剂的再生方法
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CN101754808A (zh) 2010-06-23
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